Abstract: Recent investigations within Cathole Cave have revealed several rock engravings that date from the Upper Palaeolithic including a stylised cervid, possibly a reindeer and, as yet indistinguishable engravings above and below the cervid.In advance of the erection of a protective steel grille in 2014, several archaeological trenches revealed evidence of anthropogenic and palaeozoomorphic activity which probably dates from a period when much of the northern and western parts of the British Isles was covered by ice. In November 2010, one of the authors (GHN) discovered the presence of a possible haematite (Fe203) spread that occupied a small section of the western wall of the main gallery of the cave.This spread was either the result of natural secretion from the substrate or it was applied via human agency.No other possible haematite spreads existed within this particular cave, although haematite is common throughout the limestone caves of the Gower Peninsula. In 2015 the Welsh heritage agency Cadw awarded a generous grant for the possible haematite spread to be sampled and chemically analysed, and for an overlying speleothem coat to be dated using uranium-series disequilibrium methods.This paper reports on the fieldwork and the first phase of laboratory research that included Raman Spectrometry, Scanning Electron Microscope analysis (SEM) and thin-section analysis on samples of loose substrate.The results of this phase of work confirm that the samples taken from Cathole Cave may be the result of pigment application.